Paper P507

21 rue dArtois, F-7508 PARIS http://www.cigre.org

Cigr 2009 6th Southern Africa Regional Conference

QUALITY ASSURANCE OF INSULATING OIL FOR USE IN NEW TRANSFORMERS

A. LOMBARD Eskom Enterprises (South Africa)

SUMMARY
Technical standards form the basis for insulating oil purchases. The procurement process commences with the issuing of tenders which incorporates technical specifications. Within Eskom these technical specifications are compiled by experts from the various line groups and supporting functions. The specifications are compiled based on international standards, as well as the inclusion of specifics derived from company experience and requirements. In most cases, very limited testing are performed to establish conformation of oils to standards at point of delivery and the end user are reliant upon the supplier information and documentation. These practices put the end user at risk, especially when a number of role players are involved in the handling and storage of the oil. Quality assurance testing becomes very necessary prior to oil acceptance, not only to ensure that the correct product is delivered, but also to ensure that the oil was not exposed to contaminants during the process of transportation, transfer and storage. This paper discusses a number of case studies relating to problems that were experienced, as well as new testing criteria that had to be established in order to ensure product conformance to the purchase specification against which the oil was initially accepted. The case studies cover particulate contamination, reduction of dissipation factor and interfacial tension of the oil that were experienced as a result of exposure to unknown sources during transportation and storage of oil. It also covers a case study where the presence of trace amounts of silicone oil contamination was caused due to the usage of new flexible storage bags. This paper attempts to make the end users aware of the risks that could be faced if a quality assurance program to evaluate incoming oil is not in place, as well as the advantages of such a program to enable the end user to affect the quality assurance process as agreed to during the tender is actually adhered to by the supplier.

KEYWORDS
Transformer oil, quality assurance, QA, testing

annelie.lombard@eskom.co.za

INTRODUCTION Utilities such as Eskom compile technical standards that form the basis for insulating oil purchases. The procurement process commences with the issuing of tenders which incorporates technical specifications. The tenders may be issued as a requirement for free oil - that is oil to be used for topping up, maintenance etc. or the oil requirements may be included in the purchase documents of power equipment such as a transformer. The specification forms the basis of a tender and suppliers will offer products that they feel will meet the clients requirements. Within Eskom these technical specifications are compiled by experts from the various line groups and supporting functions. The specifications are compiled based on international standards, as well as the inclusion of specifics derived from company experience and requirements. During the purchase of new equipment, the oil will be as per manufacturers specification unless a client specifies a different requirement, subject to the manufacturers approval. The oil normally arrives in the country on a sea vessel from which it is pumped via pre-cleaned and only in some cases, dedicated pipelines to a shore tank. The oil may be stored in the shore tank for days or months, depending on the demand. From the shore tank the oil will be transferred via pipelines to road tankers (not dedicated insulating oil tankers in most cases). The tankers will transport the oil to site. At site the oil may be directly pumped into the transformer. The oil will only be pumped into holding tanks or bags on site if the client specifies that a number of compliance tests need to be performed prior to filling the transformer. In most cases, very limited testing are performed to establish conformation of oils to standards at point of delivery and the end user are reliant upon the supplier information and documentation. These practices put the end user at risk, especially when a number of role players are involved in the handling and storage of the oil. Quality assurance (QA) testing becomes very necessary prior to oil acceptance, not only to ensure that the correct product is delivered, but also to ensure that the oil was not exposed to contaminants during the process of transportation, transfer and storage. SPECIFICATION AND REQUIREMENTS A client may require oil that conforms to a specification such as indicated in Table 1 below. The suppliers will offer a product that they feel meet the clients requirements. The oil would initially be tested during batching at the refinery for most of the criteria listed on the clients specification. In most cases it has been observed that the full test set is not performed by suppliers on batching of the oil. From the refinery the oil will only be checked prior to loading onto the sea vessel, at point of off loading into the shore tank, prior to loading and after loading into the road tanker. If the client insists some checks specified may be performed prior to filling of equipment. In most cases the intermediate checks only include checking of the dielectric strength, moisture, tan delta and appearance. On transfer into the customers equipment, if the client does not specify a testing protocol, the oil may only be checked for dielectric strength and moisture. Based on some of the case studies discussed later, a testing protocol for prior to filling has been compiled by Eskom that includes twelve of the tests listed in Table 1. The tests selected in Table 2 were decided upon due to merit of importance as well as characteristics that may be detrimentally affected by contaminated pipelines, tanks and tankers. The list of tests as well as acceptance criteria is given in Table 2 below.

TABLE 1: Recommended limits for oil properties of new (virgin) inhibited oils (Type I).
Oil Unit Specification Reference and/or test method

Oil type Colour Inhibitor Appearance Density @ 20 C Kinematic viscosity @ 40 C Flash point Pour point Aromatic content Total fufural and furans Polyaromatic hydrocarbons Aniline point Interfacial tension @ 25 C Neutralization value Corrosive sulphur Moisture mg/kg kg/dm3 mm2/s C C % mg/kg % C mN/m mg KOH/g ISO units %

Naphthenic (Type I) Inhibited 0.5 max. Inhibited (see Anti-oxidant additives) Clear, free of sediment and suspended matter 0.895 max. 12 max. 140 min. 21 max. 6 to 14 max. 0.1 3.0 max. 63 to 84 40 min. 0.015 max. Non-corrosive 10 max. 20 max. (2) 10 max. (3)
(1)

ASTM D1500 IEC 60666 ASTM D1500/ISO 2049 ISO3675/ISO12185 or ASTM D1298 ASTM D445/ISO 3104 ASTM D93/ISO 2719 (closed cup) ASTM D97 ASTM D2140/IEC 60590 IEC 61198 BS2000 / IP 346 ASTM D611 ASTM D971 IEC 62021-1 IEC 62535 IEC 60814 and ASTM D1533

Anti-oxidant additives Oxidation stability RBOT Dielectric strength

% by mass minutes kV/2,5 mm

0.4 max 220 min 70 min. 60 min. (2) 70 min. (3)

(1)

IEC 60666 ASTM D2112 (RBOT) IEC 60156

Dissipation factor @ 90 C Gassing tendency Maximum particulate contamination per 100 ml mm /min Particule size > 5 m Particule size > 15 m
3

0.005 max. +5 2000 particles 250 particles or 11/8 (ISO rating) (3) 130 000 particles 16 000 particles or 17/14 (ISO rating) (2) Not detectable Not detectable

BS 5737 or IEC 60247 IEC 60628 (Method A)/ASTM D2300 ISO 4406 (2000)/IEC 60970/IEC 60422

Silicon/silicone Content Polychlorinated biphenyl

ppm mg/kg

ASTM D6595 IEC 60619/EPA 600/ASTM D4059

NOTE 1: Prior to transportation NOTE 2: On delivery NOTE 3: Prior to filling Table 2: Recommended limits for oil properties of new (virgin) inhibited oils

1 2 3 4 5 6 7 8 9 10 11 12

Test criteria FTIR ( oil type verification) Water content Dielectric strength Dielectric dissipation factor (Tan delta) Interfacial tension Test for PCB Acidity Test for silicon (RDE) Corrosive sulphur Sludge Appearance Particle analysis

Acceptance criteria Depends on oil ordered <10 ppm >70 kV < 0.005 > 40 mN/m Non detectable > 0.01 mg KOH/gram oil < 2 ppm A negative result Non detectable Clear from sediments and suspended matter As per ISO 4406 (2000) - 17/14 ISO rating

TESTING In general, the electrical characteristics of insulating fluids are influenced by the intrinsic properties of the fluid, the presence of water and particles as well as the presence of dissolved polar compounds. Moisture and particles mostly influence the dielectric breakdown voltage, whereas the power factor and the resistivity are impacted upon more by dissolved polar compounds. INTERFACIAL TENSION New oil should have a high interfacial tension (IFT) value, which will decrease with the use of the oil. The interfacial tension of a mineral insulating fluid is related to the deterioration or oxidation of the oil. The oil is essentially a non-polar saturated hydrocarbon, however when the oil ages, oxygenated species such as carboxylic acids, which are hydrophilic, are formed. Contamination of products that are polar would thus also have an effect on the IFT. Prior to energising, the oil should have an IFT value > 35 mN/m. Tan Delta or Dielectric Dissipation Factor The Tan Delta or Dielectric Dissipation Factor test measures the loss angle or percentage of current that leaks through the oil under a high voltage stress in a test cell. This factor is dependant upon the amount of ions, which are a by-product of oil degradation, present in the oil. New oil should have a very low tan delta value. This value will, however, increase with the use of the oil. Water will not directly affect this property, but might form stable complexes, which will give higher tan delta values. As the oil ages, oxidation will cause the tan delta to increase. Sludge and Sediment Transformer oil consists of approximately 2900 hydrocarbons of which 2-35% is aromatic. The greatest factor in the formation of sludge is the oxidation of the transformer oil. Sludge is a resinous polymeric substance that becomes insoluble in transformer oil. It is partially conductive, hygroscopic and is a heat insulator. Sediment in transformers is normally made up of particulate contaminants that have precipitated out of the oil. Sources of contamination are created during the manufacture, maintenance activities, degradation of the cellulose insulation, or normal operation of the transformer. Other particles are metal shavings from abrasions inside the unit, maintenance, repair work, or transformer construction, shot-blast from cleaning, varnish chips, paint chips and carbon.

MOISTURE CONTENT Moisture is usually present in the oil as free moisture, in a soluble or dissolved form, or when adsorbed by polar ageing products and is then called bound water. It has been found that as temperature increases, some bound water can be converted into soluble water. Moisture is normally attracted to very dry oil and any humidity in the air will affect the results. If tankers do not have breathers, or the oil is not transported under vacuum, the moisture content will increase and the oil will have to undergo filtration prior to filling. Acidity or Neutralisation Value The neutralisation value of the oil is a measure of the presence of acidic compounds in the oil. An increase in the neutralisation number will normally indicate oxidation of the oil. The presence of acids is negligible in new or virgin oil, however may be affected if contaminated. Dielectric Strength Dielectric strength can be defined as the ability of oil to withstand electrical stress. Moisture, particles and in particular particles in the presence of dissolved moisture, may migrate to regions of high electric stress. Fine particles may be dispersed or agglomerate and particle chains may develop. Particles may even cause partial discharges to develop in the oil which will decrease the breakdown voltage of the oil. Particles can originate from various sources: Cellulose fibres trapped in the transformer after manufacture or repair. Metal particles from abrasion pump wear or manufacture and assembly. Filter particles, originating from oil processing. Silica gel dust from the breathers. Small flakes from varnishes and other coating materials.

Acceptable values prior to energising the transformer should be as high as possible. Larger utilities tend to prefer values of equal or above 70 kV. Corrosive Sulphur Some concern has been raised regarding the corrosiveness of sulphur in transformer oil and the impact this has on the transformers insulation system. Sulphur in the oil reacts with the copper (conductors) under high temperature conditions, forming copper sulphide. This formation is exacerbated by low oxygen content in the oil such as when conservator bladders are installed on the transformer. Copper sulphide is conductive, adheres to most surfaces (importantly, the paper insulation) and does not dissolve in the oil. Deposits of this harmful compound may be responsible for several transformer failures seen over the years. Oil is not the only material that contains sulphur. Sulphur compounds are also present in the gaskets, some water-based glues, copper and paper insulation used in the manufacture of transformers. Sulphur can also be introduced into the transformer through accidental means such as through the use of incompatible hoses. PARTICLE CONTAMINATION Insulation problems involve predominantly impairment of insulation conditions in service. A general ageing problem is the accumulation of conductive and polar particles in oil, as well as the deposit of these particles on the surface of the insulation material. Particles in oil decrease both the AC and DC

breakdown voltages of the oil. The breakdown voltage is dependent on both the particle size and the conductivity of the particles. With conducting metal or partially conductive particles such as carbon and wet cellulose fibres, the decrease of the breakdown strength is significantly greater in the case of direct voltage. Small particles can agglomerate to form larger particles. These larger agglomerates can again break up under mechanical and electrical stresses to form smaller particles, resulting in contradictory test results obtained in some laboratory analyses. IEC 60422 has published the table below, which indicates acceptable levels of particles in insulating fluid at various stages of the oil handling process. ISO CLASS Maximum counts per 100 cm3 5m 15m
250 32

Conta minati on level

Nil

Typical occurrence

Dielectric strength

Recommended action

Up to 8/5

9/6 10/7

1000

130

Low

11/8 15/12

32000

4000

Normal

IEC requirement for sample bottle filled with solvent Excellent oil cleanliness during factory acceptance test Contamination level for transformers in service

Good Poor

No further action Identify type of particles Dirt or dry cellulose. Repeat dielectric test with procedure appropriate for particles. Identify type of particles. Check moisture. Filtering may be considered. Recheck particle count. Repeat dielectric test with procedure appropriate for particles. Investigate source of particles Filtration or replacement is strongly recommended.

16/13 17/14

130000

16000

Marginal

Contamination level found in transformers in service

Good

Marginal

18/5 and above

High

Contamination level rare and usually indicative of abnormal operating conditions

Good

Marginal

POLYCHLORINATED BIPHENYL (PCB) PCB is the generic term for a broad class of fire-resistant synthetic insulating liquids composed of polychlorinated biphenyls, sometimes with the addition of polychlorinated benzenes. PCB is a synthetic substance not known to occur naturally. It was first described in technical literature in 1881 and commercial production commenced in the late 1920s. PCB is any one of a number of 209 possible variations in which one to ten chlorine atoms are attached to a biphenyl group. PCB was produced under a number of trade names by a number of manufacturers. PCB is soluble in most organic solvents, but insoluble in water. It is denser than water and when added to water will sink to the bottom. Most PCB mixtures are non-volatile at a temperature around 40 C, with a flash point at a temperature exceeding 300 C. Overheating of electrical equipment can produce emissions of irritating and toxic vapours. PCB is completely destroyed under extreme heat conditions, such as in temperatures exceeding 1 100 C. PCB can only be found in equipment where it had been intentionally placed or accidentally mixed in. The presence of PCB in mineral insulating oil is due to contamination during top-ups, purification, filtration or oil replacement. PCB is listed on the United Nations' Persistent Organic Pollutant (POP) list and is a banned substance.

ANTI-OXIDANT (INHIBITOR) PRESENCE BY MEANS OF FOURIER TRANSFORM INFRARED (FTIR) ANALYSIS An inhibitor or antioxidant additive has the effect of slowing down the oxidation of oil and thus the formation of byproducts such as sludge and acids. It is important to know whether and in what proportion antioxidant additive has been added in order to monitor additive depletion rate during service. 2,6-di-tertry-butyl-paracresol (DBPC) is the most commonly used antioxidant, but others may also be used. DBPC also referred to as butylated hydroxytoluene (BHT), is used as an oxidation inhibitor (antioxidant) in oils, plastics, food and other materials. The recommended addition of 0.3% (by weight) to new and used insulating oils is recommended. The presence of inhibitor as well as any obvious contaminants or oil property deviation may be checked by FTIR, which provides a quick scan method for this purpose SILICON/SILICONE Silicon, a naturally occurring substance (sand/dust) often contaminates insulating oil, but is not harmful to the unit. However, silicone oil contamination causes excessive foaming under the right conditions. For large power transformers that use forced oil cooling this may be a problem with cavitation on the forced oil cooling pumps. New oil or oil that was stored in rubber bags (especially new bags) may be contaminated due to the presence of low level silicone based releasing agents used in the manufacturing process of the bags. The presence of silicon may be checked with instruments such as Ion Coupled Plasma (ICP) or Rotating Disc Emission Spectroscopy (RDE). The presence of silicon does not automatically imply silicon oil contamination. This should be confirmed by means of foaming analysis. CASE STUDIES As mentioned earlier Table 2 were compiled based on merit of importance as well as characteristics that may be detrimentally affected by contaminated pipelines, tanks and tankers. Some of the tests were incorporated based on past experience where problems in the field were Case Study 1: During the installation of a new generator transformer, filtration of a batch of new oil, totalling 100 000 litre that was stored in rubber bags, foamed excessively. The laboratory became involved in the identification of the problem. Prior research as well as experience with foaming oil limited the cause down to the presence of low levels of silicone oil. The laboratory confirmed the presence of silicone oil as well as excessive foaming by means of elemental analysis and the foaming tendency test. Following a lengthy investigation by means of elimination of every possible source in the oil process, the rubber bags were found to be the root cause of the problem. This was established when the rubber manufacturer confirmed the use of silicone oil as a releasing agent in the manufacturing process of the rubber.

Case Study 2: A consignment of oil to one of the Transmission stations were tested and found to fail the IFT as well as the tan delta test. It was suspected that this batch of oil was possibly contaminated with some solvent during storage. This oil was stored in shore tanks previously not dedicated to oil. It was decided to check the flash point of the oil as this would confirm this theory. The oil flash point was established at approximately 20C lower than anticipated, which thus confirmed the hypothesis. Case Study 3: Oil was delivered to site for a new installation in Transmission. The oil failed both the dielectric strength as well as the particulate analysis. In order to identify the source of contamination the supplier submitted their retained samples prior to transportation. These samples passed both analyses. The initial oil was filtered and particles were visible under the microscope. The particles could not be identified in this manner and the filter paper containing the particulates was submitted for electron microscope scanning. This analysis revealed that the particulates were amongst other, paint flakes, iron ore, sea sand, fertiliser as well as bird feathers. The source was thus the utilisation of a visually, but not chemical cleaned tanker. Case Study 4: In this particular case a consignment of new oil failed the tan delta test. The cause of failure was eventually found to be the metal container used for sampling the tan delta. Glass containers are normally used for new or regenerated oil analysis as the tan delta is normally much lower than tan delta of in-service oil. Upon resampling in glass containers the oil was found to be conforming. Case Study 5: A new batch of oil was issued to a very remote Transmission site in the Northern Cape area. The oil in this case did not, after several samples were submitted passed the particulate analysis. The on site container was found to be contaminated and continues filtration of the oil back in the tank did not clear the debris in the bottom of the tank. Filtration of the oil to specification directly into the transformer was the only option to resolve this problem. CONCLUSION As can be seen from the case studies the quality assurance program that Eskom has instituted did on many occasions safeguarded their new equipment against oil of inferior quality. It is thus recommended that power equipment owners be vigilant on quality control of incoming oil in order to ensure that their plant will reach and perform optimally. REFERENCES 1. Lombard A, Fourie H, De Klerk P, Theory, design, maintenance and life management of power transformers: Condition-based monitoring of oil/paper insulation systems, Eskom Power Series Volume 5, Chapter 8, 2008. Eskom Specification 32-406, Mineral insulating oils (uninhibited and inhibited) Part 1: Purchase, Management, Maintenance and Testing. Lombard A, Particle analysis Why has it been included in NRS 079-1: Mineral

2. 3.

insulating oils (uninhibited); purchase, management and test. Energize magazine, September 2006.